Potassium Carbonate → Ethyl (3-amino-6,8-dioxo-7-propyl-4H,6H-pyrimido[6,1-b][1,3]thiazine-2-yl)carboxylate

HRID 1090652ノート

反応式

HRID 1090652 の反応式
Cl[C:2]1[N:7]([CH2:8][C:9]#[N:10])[C:6](=[O:11])[N:5]([CH2:12][CH2:13][CH3:14])[C:4](=[O:15])[CH:3]=1.[C:16]([O:20][CH2:21][CH3:22])(=[O:19])[CH2:17][SH:18].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:10][C:9]1[CH2:8][N:7]2[C:6](=[O:11])[N:5]([CH2:12][CH2:13][CH3:14])[C:4](=[O:15])[CH:3]=[C:2]2[S:18][C:17]=1[C:16]([O:20][CH2:21][CH3:22])=[O:19]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12185Ethyl ThioglycolateHCID 150275436-Chloro-1-cyanomethyl-3-propylpyrimidine-2,4(1H,3H)-dione

生成物 1

HCID 15027666Ethyl (3-amino-6,8-dioxo-7-propyl-4H,6H-pyrimido[6,1-b][1,3]thiazine-2-yl)carboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 6-chloro-1-cyanomethyl-3-propylpyrimidine-2,4(1H,3H)-dione (1.5 g), ethyl thioglycolate (0.88 g) and potassium carbonate (1 g) in ethanol (30 ml) was refluxed for 15 hours. The reaction solution was concentrated to dryness, and the resulting residue was purified by column chlomatography on silica gel. The resulting crude crystals were recrystalized from ethyl acetate-hexane to give colorless plates (0.23 g, 11%).

後処理

  1. concentrationThe reaction solution was concentrated to dryness
  2. customthe resulting residue was purified by column chlomatography on silica gel
  3. customThe resulting crude crystals were recrystalized from ethyl acetate-hexane
  4. customto give colorless plates (0.23 g, 11%)

出典と根拠

ORDレコード
ord-c0539ff182a64942881b864be5abe4e6
出典データセット
uspto-grants-1992_01
特許番号
US05082838

反応ノート

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